Hop on the cannabinoid express!

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Interesting. I know two chemists and an engineer from my miniscule spheroid who have recently joined the marijuana extraction industry here in Colorado. Crimony, it makes me wonder what my problem is. Alright, it turns out that’s easy to explain. I really dig reaction chemistry and thermo, you know, real sciency stuff. Not much of that in the retail or wholesale extractives business. I have this suspicion that it will soon – if not already – be corporatized, IPO’d, and raced full throttle by scheming finance MBA’s like every other growth business. They can have it. Capitalism is like a stomach- it has no brain. All it can do is endlessly demand more.

Gravitationally Initiated Tourette’s

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After another tedious weekly teleconference our group adjourned and stood up from the table in the conference room.  I was furthest from the door but my normally rapid pace put me in the lead to exit. All at once mid-stride, just as my rearward foot began to move forward, it caught a phone cord that became taut instantly. Consider that a walking stride is a series of balance/off-balance conditions where the walker is constantly catching his/her balance. I had been caught off-balance at the wrong moment in my step.

My recollection of that falling moment brings to mind the droll voice of the bowl of petunias in The Hitchhiker’s Guide to the Galaxy.  Resigned to its fate, its final lament is “Oh no, not again.” I can relate.

Mid-fall my lips came within a hairs breadth of landing face first on an armrest. Luckily I hadn’t shaved that day so I actually had that hairs breadth.  On impact with the carpeted floor my first emotion was one of anger. I had successfully negotiated the cords for nigh on eleven years. But this day it was not to be. This day I would tip like a sack of dirt in front of a room full of colleagues.

After a moment on the floor I spouted an incredulous “Mother F**ker!!“ followed by an equally enthused “Son of a B*tch!!” Truth be told, it was an utterly sincere cleansing of my dismay. My screens were down and the profanities leapt into the ether. After a few awkward moments I got up and repaired to the solitary confines of my office.

Later I jokingly apologized for my “gravitationally-induced Tourette’s.” I gathered that the unexpected outburst had provided a welcome bit of mirth after a highly technical meeting.

 

What’s up with the Sigma-Aldrich catalog?

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In the course of my forays into chemical sourcing or searching for data, I have begun to notice something about product entries in the online Sigma-Aldrich catalog. I’m finding that since the acquisition of Sigma Aldrich by Merck KGaA, MilliporeSigma as it is now known, many of the compounds that I find listed say the product has been discontinued. Is it just fortuitous, or is it not? Is the catalog collection being trimmed?

Have I been collecting data? Pffft! Of course not, silly. It’s just the subjective experience of having found few if any Aldrich catalog entries labeled as discontinued over the past few decades. Recently I’m landing on the pages of discontinued products. Hmmm.

Over the many years, buying reagents from Aldrich has saved countless chemist-days in lab productivity. In fact, the availability of their huge collection of chemicals has driven the direction of much research out there based simply on the availability of reagents for purchase.

I blame the MBA’s. This has the smell of overly smart weasels marketing people.

Ionospheric Bow Waves Caused by August, 2017, Eclipse

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A recent paper (free) in Geophysical Research Letters reports the discovery of long anticipated ionospheric disturbances caused by the passing of the moon’s shadow over the earth during an eclipse. The paper, submitted by the MIT’s Haystack Observatory, reports the occurrence of ionospheric bow waves associated with the shadow ground-track of the August, 2017, North American eclipse.  The online source, MIT News, summarized the discovery.

 

Life With an RC1

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I’ve been using a Mettler-Toledo (MT) RC1e reaction calorimeter for about 6 years. Our system came with MT’s iControl software, RTCal, and 2 feed pumps with balances. Overall it has proven its worth for chemical process safety and has helped us understand and adjust the thermal profile of diverse reactions. Like everything else, MT’s RC1e has many strengths and a few weaknesses.

The RC1e’s mechanical side seems reasonably robust. Our instrument sits in a walk-in fume hood resting on a low lab benchtop supported by an excess of cinder blocks- it is a heavy beast. During installation we discovered that the unit would not achieve stable calibration with the hood sash closed. The control box mounted on the instrument didn’t work properly on installation. After a trip to the repair shop, the box was returned as functional but without finding the fault.

Recently we had a mixing valve fail in the heat transfer plumbing, resulting in down time. Diagnosis of this was unsuccessful over the email and phone, necessitating a service call. Parts may not be inventoried in the US and consequently must come from Switzerland. Expect Swiss prices and less than snappy delivery. Hey, it’s been my experience.

Addendum, 5/4/22:  After a nearly 1 year period of down time the RC1 was reinstalled at another location. Due to temperature regulation problems after the move, a technician from MT visited and repaired the instrument. It turns out that swapping one of the hot legs on the  208 3 phase feed for another can cause the stir motor to reverse direction. A relief valve related to the heat transfer system had failed in the partially open condition. It was fixed and the instrument now performs as expected.

Addendum 2, 6/10/22: The RC1 has failed again. The “fix” didn’t work. Same problem as before. Maybe in the next repair they’ll replace the bloody valve rather than just “unstick” it. Unrelated gripe- Getting parts from Mettler-Toledo in Switzerland has been frustrating. They have always been very slow. So much for Swiss efficiency.

A chiller unit is required for RC1 operation and can add 15-30 k$ to the setup cost. Users will have to contend with the loss of floor/hood space in the lab for the chiller and RC1. The chiller must be powerful enough to contend with the exotherms that may be generated in the instrument. Chillers can take many hours to get down to the set temperature. Given that RC1 experiments can also be lengthy, plan accordingly. Our (brand new Neslab 80) chiller requires nearly 2 and 1/2 hours to get from +20 C to -20 C, which is the lower chiller temperature we use, depending on the reaction chemistry. For reactions that are on the sporty side, we’ll drop the chiller to – 50 C.  This is near the  minimum temperature for the water-based chilling fluid we use. Early on I opted for an aqueous potassium formate solution with a very low freezing point. The instrument comes with a panic button that switches to full cooling in an emergency.

The chiller required the wiring-in of a dedicated single-phase 208 VAC circuit. With the chiller using single-phase and the RC1e using 3-phase 208 VAC, it is important to assure that one cannot inadvertently connect into the wrong power circuit (idiot proofing). The chiller plug design should already prevent this. It is critical that the electrician is alert to this and does NOT jury-rig the plugs to use the same style of connectors because he has only one style in the parts bin.

Some comments on the collection and interpretation of RC1 thermograms.

  • It is critical that those who request RC1 experiments understand the limitations of the instrument. For instance, we use a 2 Liter reaction vessel with a 400 mL minimum fill volume. Refluxing is not allowed owing to the huge thermal noise input from the reflux return stream. Special equipment is said to be available for reflux.
  • Experiments must be carefully designed to elicit results that can answer questions about feed rates and energy accumulation.
  • Like many instruments, the RC1 needs a dedicated keeper and contact person for inside and outside communication. A maintenance logbook should be kept next to the instrument if for no other reason than to pass along learnings from previous issues.
  • If thermokinetic measurement is part of your organization’s development SOP, someone on staff should be reasonably familiar with some chemical thermodynamics. That can be a chemical engineer, as may often be the case.
  • The users of thermal data are likely to need help with interpretation of the results. Be prepared to offer advice on interpreting the data, taking care not to over-interpret. If you don’t know, say so. It is easier to claw back “I don’t know” than “yeah, go ahead and do that …”.
  • Do not be anxious to singlehandedly bear the weight of responsibility for safety. Safety is a group responsibility.
  • Be curious. How do the insights and learnings from the data translate into best practices? What changes, if any, can the process chemists make to nudge the process for better safety and yields? A credible specialist in RC can make comments or ask questions that lead to better discussions on thermal hazards. Be a fly in the ointment.
  • Never forget that a reaction calorimeter is a blunt instrument for the understanding of a reaction. An RC1 thermogram is a composite of overlapping solution-phase phenomena. Interpretation of results can be greatly refined by pulling timely aliquots for NMR, GC/MS, or HPLC analysis.
  • A database should be constructed to collect and immortalize learnings from all safety work and RC1 learnings fall into that group.

There is the question of who collects and presents the data. An engineer or a chemist? Engineering thermodynamics is a big part of a chemical engineer’s education and skill set. As a plus, an engineer can take thermal data and apply it to scale-up design for safety and sizing of equipment and utilities. You know, the engineering part. On the down side, there may not be many chemical engineers who are comfortable with doing reaction chemistry.

Do not be anxious to singlehandedly bear the weight of responsibility for safety. Alpha males- are you listening??  Safety is a group responsibility that should originate from a healthy group dynamic.

There’s a good argument for a chemist to conduct RC experiments as well. A trained synthesis chemist is qualified to conduct chemical reactions within their organization. That includes sourcing raw materials, handling them, running the reaction, and safely cleaning up the equipment afterwards. But interpreting RC1 data has a physical chemistry component. In my experience, run of the mill inorganic/organic synthesis people may have seen PChem as an obstacle rather than a focus in their college education. Their skill set is in instrumental analysis like NMR and chromatography, mechanisms, and reaction chemistry. I would recommend having a PhD chemist in a leadership role when calorimetry is a key part of a busy process safety environment.

Safety data can be collected and archived all day long. The crucial and often tricky part is how to develop best practices from the data. I would offer that this is inherently a cross-disciplinary problem. Calorimetric data from reaction chemistry can be collected readily, especially with the diverse and excellent instrumentation available today. Adiabatic temperature rise, ΔTad, is a key measurement. A lab group may be interested in the maximum (adiabatic) heat rise for a given reaction. A smooth and efficient technology transfer from lab to plant happens when good communication skills are used. Yes, SOP’s must be in place for consistency and safety. But the positive effect of individuals who have good social skills and are prone to volunteering information cannot be underestimated.

A Pox on the House of Microsoft

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An automated Windows update disrupted my life today. It swooped in overnight like a winged wraith, did its dark deeds, and flapped quietly back to the dank hole from whence it came. My RC1 data may yet reside unscrambled on the disk drive, but it lies orphaned from the mother iControl application which mockingly professes no recollection of 18 hours of sweet data lovingly produced. The curs in IT can only “tsk, tsk” in their antiseptic way while bobbing pointed heads in faux dismay. Another first-world difficulty uncovered for all to see.

Cripple Creek Gold

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A Blacksmith shop is all that remains of Anaconda, Colorado.

A Blacksmith shop is all that remains of Anaconda, Colorado.

The discovery of gold in the early 1890’s west of Pikes Peak at Cripple Creek was the last major gold rush in Colorado. This discovery coincided with the repeal of the Sherman Silver Act which compelled the government to guarantee a price for silver. The repeal of the Sherman Silver Act led to an immediate collapse in silver prices and the crash of virtually all silver mining operations.  As a result, miners in the area made their way to Cripple Creek for newly discovered gold.

Today many of the valleys around Cripple Creek and Victor are largely regrown and quiet. Little indication remains of the towns and mills that once covered the area. Many mining towns were consumed by fire and a few were rebuilt. Once town left to extinction is Anaconda.

In the winter of 1904 a fire consumed the mining town of Anaconda. Today, all that remains is the shell of a blacksmith shop. This abandoned building sits at the end of the line on the Cripple Creek and Victor Narrow Gauge Railroad (CC&V).  Near Anaconda were a number of significant mines- the Mary McKinney, the Doctor Jack Pot, the Chickenhawk, the Anaconda mine and others.

Nearby is the Mollie Kathleen mine which is open for tours. This tour involves piling into a small-man lift and dropping 1000 ft into the mine. This puts you below the level of Cripple Creek, located in the valley below. If you are very lucky, the big open pit gold mine on the other side of the mountain will do some bench blasting while you are down there. It’s very exciting. The mountain between the big CC&V mine and the Mollie Kathleen is riddled with shafts and drifts.

The Cripple Creek & Victor Gold Mine east of Cripple Creek is a large open pit gold mining operation run by Newmont Mining Corporation. The gold in the mine is highly disseminated in microscopic form and is recovered by cyanide heap extraction. The CC&V deposit is the remnant of an extinct volcano that is highly brecciated. Hydrothermal water has extracted and transported gold throughout the throat of the volcano and into the surrounding rock. However, much of the gold (ca 30 %) is tied up as gold telluride, AuTe2, also known as calaverite. The gold in calaverite cannot be extracted with cyanide and must be left behind. The tellurium can be removed by roasting and burning off the oxide, but this is highly polluting. This gold formation is where the famous Cresson Vug was located. It was a cavity in the formation that yielded 60,000 troy ounces of gold.

CC&V Steam Engine

CC&V Steam Engine

The CC&V railroad is a modest tourist attraction located on the outskirts of Cripple Creek. The line has several operating steam locomotives that take passengers on a 45 minute trip into the countryside. Our engineer estimated the horsepower of the engine above to be ca 20 hp.  Narrow gauge rail was popular in mountainous areas as opposed to standard gauge owing to the ability to negotiate a tighter turn radius.

On Nuclear War With the DPRK

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The electronic news world is a colossal hodgepodge of media jumping on anything new and “compelling”. The weekend’s compelling news du jour is Ret. Adm. Mike Mullen‘s comments on the likelihood of nuclear war with North Korea (DPRK). As a retired admiral and chairman of the Joint Chiefs, Mullen is a strategic thinker. These days he is very pessimistic of the US finding a peaceful way forward with the DPRK.

Taken alone, this view could be ignored as an outlier. But against a backdrop of other seemingly credible reports, Mullen’s worry could be taken as another indicator of the tempo of concern within much of DC. Consistent with Mullen’s worry is a lengthy 12/14/17 interview with Senator Lindsey Graham written by Uri Friedman at The Atlantic. Graham is an opinion leader on the matter of the DPRK. The article is well written and I must highly recommend it.

The frothy part of this DPRK boil-up is talk of nuclear conflict. The language that I have heard does not distinguish the various scenarios of how a nuclear war would unfold on the Korean Peninsula. One thing that was made clear by Graham in the Atlantic article is that there could be no limited strike on the DPRK. I assume it means defensively or otherwise. Any attack on the North, nuclear or conventional, would have to result in the complete collapse of the Kim regime.

The US military develops and refines war plans in preparation for any contingency. But, I’m curious how the psychological impact of the use of nuclear weapons will play in the various war cabinets of the world. After all, the nuclear-bomb genie has been kept in the bottle since August, 1945. Will a first use on or by the DPRK lower the threshold for other nuclear states?

A nuclear weapon married to a missile is a highly engineered machine that is at the apex of multiple military technologies. Expertise and a minimum of infrastructure in metallurgy, nuclear physics, chemistry, propellants, and delivery vehicle technology is necessary for accurate execution of a strike. For the DPRK to maximize the punch of its limited nuclear armaments, a strike relying on accurate delivery of a nuclear war shot to a remote or hardened target would require their leadership to gamble on layers of unproven or unrefined technology. The Kim regime may be a political malignancy, but they are not stupid.

Suppose the DPRK is able to strike some important targets with its nukes. Surely some in the North’s command know the consequences to follow. Decapitation of its leadership and annihilation of its war making capacity are a certainty.

For the US, the use of a nuclear war shot on the DPRK is not an inevitable result of physics like the apple that fell on Newton’s head. A release from the US nuclear arsenal is a choice and thus psychological in both application and long term consequence. Would a US nuclear response to a nuclear strike- anywhere-  by the DPRK make sense for the US in the subsequent post-war world?

The last big war, WWII, started conventional and ended nuclear.  Since then, the threat of mutual nuclear conflagration has helped to keep the peace by serving as a deterrence. Mutual Assured Destruction, MAD, is credited, superficially a least, with keeping armed conflict a strictly chemical explosives activity. What happens to the ground under the psychological pedestal supporting MAD when a nation-state uses nuclear weapons thinking it could win a conflict? How would the various national policies on first use change across the world and what do the likely outcomes look like?

There are many issues that follow from conflict with the DPRK. I hope that as much energy is given to the diplomatic scene as the theatre of war.

Some useful instructions

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How to follow directions-

  1. Look at the person
  2. Say ‘OK’
  3. Do it

How to do anything-

  1. Start at the beginning
  2. Proceed through the middle
  3. Stop when finished

How to save electrical energy-

  1. When leaving an area, Turn Off the Goddamned Lights!

I’ll confess that I am especially peevish about the last instruction.

What instructions do you have to share, dear reader?

 

Time to accept that Trump is too great a liability to retain in office

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Recital.

Whereas contemplation of the lawful removal of the 45th President of the United States is a serious matter; and,

Whereas the President of the United States, Donald Trump, has displayed public behavior that can reasonably be characterized as profane, untruthful, misogynistic, and a demonstrated top-level fomenter of many of the base instincts of man; and,

Whereas the President has consistently displayed conduct, both internationally and within US borders, that is unbecoming of the top-level executive and de facto moral representative of the citizens of the United States of America; and,

Whereas the President has with malice and purpose attempted to incite foreign states with disrespect, schoolyard taunts, slander, and in the case of the DPRK, public threats of total annihilation, nuclear or otherwise; and,

Whereas the President has unilateral control over the release of nuclear war shots while, in this capacity, cultivated a mode of operation that is antithetical to US norms and traditions, and is unburdened by knowledge of the hard earned historical precedents relating to our nuclear weapons complex and decades of successful strategy pertaining to nuclear conflict and their enduring effects;

Therefore, be it resolved that the 45th President of the United States should be lawfully removed the from office by the US Congress under the terms of Section 4 of the 25th Amendment to the Constitution of the United States.

Note: This is only one of a great many possible declarations calling for the removal of President Trump. Focus your thoughts. Try writing and publishing your own.

 

Twenty-fifth Amendment to the United States Constitution

Section 1. In case of the removal of the President from office or of his death or resignation, the Vice President shall become President.

Section 2. Whenever there is a vacancy in the office of the Vice President, the President shall nominate a Vice President who shall take office upon confirmation by a majority vote of both Houses of Congress.

Section 3. Whenever the President transmits to the President pro tempore of the Senate and the Speaker of the House of Representatives his written declaration that he is unable to discharge the powers and duties of his office, and until he transmits to them a written declaration to the contrary, such powers and duties shall be discharged by the Vice President as Acting President.

Section 4. Whenever the Vice President and a majority of either the principal officers of the executive departments or of such other body as Congress may by law provide, transmit to the President pro tempore of the Senate and the Speaker of the House of Representatives their written declaration that the President is unable to discharge the powers and duties of his office, the Vice President shall immediately assume the powers and duties of the office as Acting President.

Thereafter, when the President transmits to the President pro tempore of the Senate and the Speaker of the House of Representatives his written declaration that no inability exists, he shall resume the powers and duties of his office unless the Vice President and a majority of either the principal officers of the executive department or of such other body as Congress may by law provide, transmit within four days to the President pro tempore of the Senate and the Speaker of the House of Representatives their written declaration that the President is unable to discharge the powers and duties of his office. Thereupon Congress shall decide the issue, assembling within forty-eight hours for that purpose if not in session. If the Congress, within twenty-one days after receipt of the latter written declaration, or, if Congress is not in session, within twenty-one days after Congress is required to assemble, determines by two-thirds vote of both Houses that the President is unable to discharge the powers and duties of his office, the Vice President shall continue to discharge the same as Acting President; otherwise, the President shall resume the powers and duties of his office.  Source: Wikipedia.